CN107833821A - A kind of double threeway capillary pipe spray devices of open type and its application - Google Patents
A kind of double threeway capillary pipe spray devices of open type and its application Download PDFInfo
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- CN107833821A CN107833821A CN201710881280.5A CN201710881280A CN107833821A CN 107833821 A CN107833821 A CN 107833821A CN 201710881280 A CN201710881280 A CN 201710881280A CN 107833821 A CN107833821 A CN 107833821A
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- pipe
- way pipe
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- capillary
- spray
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0404—Capillaries used for transferring samples or ions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
- H01J49/165—Electrospray ionisation
- H01J49/167—Capillaries and nozzles specially adapted therefor
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electrochemistry (AREA)
- Plasma & Fusion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a kind of double threeway capillary pipe spray devices of open type, the first three-way pipe (1) and the second three-way pipe (2) including series connection, sample channel is formed in the horizontal direction, capillary pipe spray pipe (3) is provided with the sample channel, the rear end of the capillary pipe spray pipe (3) is connected with one end of isocon (4), front end is arranged in the sample channel, blending space is formed between the right-hand member of second three-way pipe (2), the other end of the isocon (4) is connected with sample bottle (5) and waste liquid bottle (6) respectively by pipeline, first three-way pipe (1) provides device (7) with gas and is connected, second three-way pipe (2) is connected with syringe pump (8), mass spectrograph (9) is provided with the right side of second three-way pipe (8).The double threeway capillary pipe spray devices of open type of the present invention can be joined directly together with sample, in open environment can direct injected, pass through the analysans in mass spectrograph quick detection sample.
Description
Technical field
The present invention relates to the detection means of chemical substance, more particularly to a kind of double threeway capillary pipe spray devices of open type
And its application.
Background technology
Spray product is to use extensive product during we live.Product type mainly has two classes：One kind is by bottle
Gas provides the aerosol product of spraying power, a kind of to provide the spray product of power by Manual press in addition.The tool of product
Body classification is also a lot, including：Hair dyeing spraying, the spraying of use in personal care of the insecticide of agricultural and family expenses, hair-dyeing are made up
The medicinal herb spray etc. of product, traumatic injury.At present, needed for the conventional detection process of aerodynamic force spray product by sample
After being placed in low temperature refrigerator freezing, bottle is pried open, releases propellant, and then sample is carried out to extract the steps such as separation；For external force
The detection of spray product is acted on, its pretreatment process is also relatively complicated, takes time and effort.
The content of the invention
The technical problem to be solved in the present invention is to provide one kind is simple in construction, cost is cheap, open type easy to operate is double
Threeway capillary pipe spray device, it is composed in series by two three-way components, there be a spray capillary run through inside.Two three
Logical branch road can introduce gas and liquid respectively.The gas of introducing is used to dispel the liquid that atomization introduces, the small liquid pearl after atomization
The mass spectrum response of object to be analyzed can be strengthened.
It is an object of the invention to provide a kind of capillary pipe spray device docked suitable for nebulised sample with mass spectrum.
The applicable spray product type of apparatus of the present invention：1) aerodynamic force spray product (aerosol product), 2) manual force spray
Mist product (pressing spray product).
A kind of double threeway capillary pipe spray devices of open type, include the first three-way pipe and the second three-way pipe of series connection, in water
Square sample channel is upwardly formed, is provided with capillary pipe spray pipe on the sample channel, after the capillary pipe spray pipe
End is connected with one end of isocon, and front end is arranged in the sample channel, the right-hand member of close second three-way pipe, and described
Form blending space between the right-hand member of second three-way pipe, the other end of the isocon by pipeline respectively with sample bottle and waste liquid
Bottle is connected, and first three-way pipe provides device with gas by pipeline and is connected, and second three-way pipe passes through pipeline and injection
Pump is connected, and mass spectrograph is provided with the right side of second three-way pipe, and the air pressure that the gas provides device is 10~50psi,
The injection speed of the syringe pump is 5~200 μ L/min.
The double threeway capillary pipe spray devices of open type of the present invention, wherein, first three-way pipe and described second
Three-way pipe includes horizontal tube and VERTICAL TUBE, and the left end of the horizontal tube of first three-way pipe is closed using stator, right-hand member with
The left end of the horizontal tube of second three-way pipe is connected, and through hole is provided with the stator, the capillary pipe spray pipe
Rear end passes from the through hole, is connected with the isocon.
The double threeway capillary pipe spray devices of open type of the present invention, wherein, the VERTICAL TUBE of first three-way pipe is led to
Cross pipeline with gas offer device to be connected, the VERTICAL TUBE of second three-way pipe is connected by pipeline with the syringe pump.
The double threeway capillary pipe spray devices of open type of the present invention, wherein, first three-way pipe and described second
The interface of three-way pipe is 1/8 inch or 1/16 inch.
The double threeway capillary pipe spray devices of open type of the present invention, wherein, the internal diameter of the capillary pipe spray pipe is
10~200 μm.
The double threeway capillary pipe spray devices of open type of the present invention, wherein, the front end of the capillary pipe spray pipe is set
Put in second three-way pipe, the distance between right-hand member of horizontal tube of second three-way pipe is 1~3cm；Described
The right-hand member of the horizontal tube of two three-way pipes is 2~4cm apart from the distance between described mass spectrometric injection port.
The double threeway capillary pipe spray devices of open type of the present invention, wherein, it is provided with flow on the isocon
Regulating valve.
The double threeway capillary pipe spray devices of open type described in any one in the present invention are in spray product analysis detection
Application.
The double threeway capillary pipe spray device differences from prior art of open type of the present invention are：
The double threeway capillary pipe spray devices of open type of the present invention can be joined directly together with sample, can directly be entered in open environment
Sample, pass through analysans in mass spectrum quick detection sample.Present invention firstly provides the double threeway capillary pipe spray devices of open type, sheet
The device of invention is applied to nebulised sample direct injection analysis, and apparatus of the present invention can be by introducing H+Or derivatization reagent is to carry
The response of high analysans.
The double threeway capillary pipe spray devices of open type of the present invention and its application are described further below in conjunction with the accompanying drawings.
Brief description of the drawings
Fig. 1 is the structural representation of the double threeway capillary pipe spray devices of open type of the present invention；
Fig. 2 is the matter that isoprocarb in insect aerosol is detected using the double threeway capillary pipe spray devices of open type of the present invention
Spectrogram (parent ion m/z 194.3)；
Fig. 3 is the mass spectrum of oestrone in the double threeway capillary pipe spray device detection spraying cosmetics of open type using the present invention
Scheme (parent ion m/z 300.2).
All English bilinguals occurred in Fig. 2 and Fig. 3 are as follows：：
Relative abundance：Relative abundance；
m/z：Mass-to-charge ratio；
Isoprocarb：Isoprocarb；
Intensity：Intensity；
Estrone：Oestrone.
Embodiment
As shown in figure 1, the double threeway capillary pipe spray devices of open type of the present invention include the first three-way pipe 1 and second of series connection
Three-way pipe 2, forms sample channel in the horizontal direction, and capillary pipe spray pipe 3, capillary pipe spray are provided with sample channel
The rear end of pipe 3 is connected with one end of isocon 4, and front end is arranged in sample channel, close to the right-hand member of the second three-way pipe 2, with the
Form blending space between the right-hand member of two three-way pipes 2, the other end of isocon 4 by pipeline respectively with sample bottle 5 and waste liquid bottle 6
It is connected, the first three-way pipe 1 provides device 7 with gas by pipeline and is connected, and the second three-way pipe 2 is connected by pipeline with syringe pump 8,
The right side of second three-way pipe 8 is provided with mass spectrograph 9.After sample, gas circuit and the tunnel of fluid path three are well mixed in blending space from
Sprayed in second three-way pipe 2, into mass spectrograph 9.The air pressure that gas provides device 7 is 10~50psi, and the injection of syringe pump 8 is fast
Spend for 5~200 μ L/min.
It is preferred scheme below：
First three-way pipe 1 and the second three-way pipe 2 include horizontal tube and VERTICAL TUBE, a left side for the horizontal tube of the first three-way pipe 1
End is closed using stator 10, and right-hand member is connected with the left end of the horizontal tube of the second three-way pipe 2, is provided with stator 10 logical
Hole, the rear end of capillary pipe spray pipe 3 pass from through hole, are connected with isocon 4.The VERTICAL TUBE of first three-way pipe 1 passes through pipeline
Device 7 is provided with gas to be connected, the VERTICAL TUBE of the second three-way pipe 2 is connected by pipeline with syringe pump 8.First three-way pipe 1 and
The interface of two three-way pipes 2 is 1/8 inch or 1/16 inch.The internal diameter of capillary injection spray pipe 3 is 10~200 μm.
The front end of capillary pipe spray pipe 3 is arranged in the second three-way pipe 2, with the right-hand member of the horizontal tube of the second three-way pipe 2 it
Between distance be 1~3cm；The right-hand member of the horizontal tube of second three-way pipe 2 apart from the distance between injection port of mass spectrograph 9 be 2~
4cm.Flow control valve is provided with isocon 4, can adjust sample size.
First three-way pipe and the second three-way pipe (the big Lip river gram of generation (Shanghai) fluid system Science and Technology Ltd.)；P-1000 types are micro-
Electrode draws instrument (Sutter companies of the U.S.)；Capillary pipe spray pipe (the sharp Feng chromatograms device Co., Ltd of Yongnian)；Bruker
AmaZon ion trap mass spectrometers (Bruker Dalton companies of the U.S.).
The device application method of the present invention：Sample bottle 5 is connected with isocon 4, and ensures its sealing.Isocon 4 its
In be passed through waste liquid bottle 6 all the way, another way is connected with the capillary pipe spray pipe 3 in double threeway capillary pipe spray devices；Double threeway hairs
Spool spraying each leads into gas circuit and fluid path.The air valve of sample bottle 5 is pressed, sample sprays, and enters double threeway capillarys by isocon 4
Pipe sprayer unit, formed and sprayed in exit.The condition of mass spectrograph 9 is set, and mass spectrum obtains corresponding signal.
Double applications of the threeway capillary pipe spray device in banned substance in detecting spray product of open type, tool in the present invention
Body application mode embodiment：
First, in insecticide isoprocarb quick detection：
Reagent and material unless otherwise specified, commercially obtain.
The first step：The making of positive
Isoprocarb is national banned pesticides, chemical abstracts 2631-40-5, molecular weight 193.2.Desinsection containing isoprocarb
Spray positive commission aerosol manufacturer Xiong Ankaichen daily use chemicals Co., Ltd makes.
Second step：Sample is connected with the device of the present invention and Mass Spectrometer Method
Pesticide spray positive is connected with double threeway capillary pipe spray devices.The internal diameter of capillary pipe spray pipe 3 is 20 μ
M, the injection port distance apart from mass spectrograph 9 is 3cm, air pressure 30psi.Mass Spectrometry Conditions are set as：Positive ion mode, capillary electricity
Press 4kV.Product aerosol valve is pressed, obtains mass spectrum response signal.
3rd step：Improve the response of analysans
Syringe pump 8 introduces formic acid solution, and fltting speed is 20 μ L/min, and atomization gas dispels atomization formic acid drop, double three
End spaces provides a large amount of H before logical capillary+, isoprocarb mass spectrum response signal can be improved, signal is as shown in Figure 2.The prison of isoprocarb
Survey parent ion is m/z 194.3, and monitoring daughter ion is m/z 151.6.
2nd, spray cosmetics in oestrone quick detection：
The first step：The making of positive
The oestrone standard liquid of various concentrations is added into the spraying toner for being free of oestrone after testing, the positive is prepared
Sample, oestrone are《Cosmetics safety hygienic practice》Cosmetics banned substance as defined in (version in 2015), chemical abstracts number are 53-
16-7, molecular weight 270.3.
Second step：Double threeway capillary quick determination methods
Spraying toner positive is connected with double threeway capillary pipe spray devices.The internal diameter of capillary pipe spray pipe 3 is 20 μ
M, the injection port distance apart from mass spectrograph 9 is 3cm, air pressure 30psi.Mass Spectrometry Conditions are set as：Positive ion mode, capillary electricity
Press 4kV.Product aerosol valve is pressed, obtains mass spectrum response signal.
3rd step：Improve the response of analysans
Syringe pump 8 introduces 100mM methoxamine derivatization reagent, and fltting speed is 20 μ L/min, and atomization gas dispels atomization
Methoxamine drop, derivative reaction occurs for end spaces before double threeway capillaries, improves the mass spectrum response signal of oestrone, and it derives
Mass spectrogram is as shown in Figure 3 after change.
Before derivatization, the parent ion of oestrone is m/z 271.3, and big by noise jamming, response is low.Filled by the present invention
Put, introduce methoxamine derivatization reagent, the monitoring parent ion selection of oestrone is m/z 300.2, and corresponding daughter ion is m/z
252.8, response significantly improves 24 times compared with underivatized.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, technical side of the those of ordinary skill in the art to the present invention
The various modifications and improvement that case is made, it all should fall into the protection domain of claims of the present invention determination.
Claims (8)
- A kind of 1. double threeway capillary pipe spray devices of open type, it is characterised in that：The first three-way pipe (1) and second including series connection Three-way pipe (2), forms sample channel in the horizontal direction, and capillary pipe spray pipe (3) is provided with the sample channel, described The rear end of capillary pipe spray pipe (3) is connected with one end of isocon (4), and front end is arranged in the sample channel, close to described Blending space is formed between the right-hand member of second three-way pipe (2), and the right-hand member of second three-way pipe (2), the isocon (4) The other end is connected with sample bottle (5) and waste liquid bottle (6) respectively by pipeline, and first three-way pipe (1) passes through pipeline and gas There is provided device (7) to be connected, second three-way pipe (2) is connected by pipeline with syringe pump (8), in second three-way pipe (8) Right side be provided with mass spectrograph (9)；The air pressure that the gas provides device (7) is 10~50psi, and the injection speed of the syringe pump (8) is 5~200 μ L/ min。
- 2. the double threeway capillary pipe spray devices of open type according to claim 1, it is characterised in that：First three-way pipe (1) and second three-way pipe (2) includes horizontal tube and VERTICAL TUBE, and the left end of the horizontal tube of first three-way pipe (1) is adopted Closed with stator (10), right-hand member is connected with the left end of the horizontal tube of second three-way pipe (2), on the stator (10) Through hole is provided with, the rear end of the capillary pipe spray pipe (3) passes from the through hole, is connected with the isocon (4).
- 3. the double threeway capillary pipe spray devices of open type according to claim 2, it is characterised in that：First three-way pipe (1) VERTICAL TUBE provides device (7) with the gas by pipeline and is connected, and the VERTICAL TUBE of second three-way pipe (2) passes through pipe Road is connected with the syringe pump (8).
- 4. the double threeway capillary pipe spray devices of open type according to claim 3, it is characterised in that：First three-way pipe (1) and second three-way pipe (2) interface be 1/8 inch or 1/16 inch.
- 5. the double threeway capillary pipe spray devices of open type according to claim 4, it is characterised in that：The capillary pipe spray The internal diameter for managing (3) is 10~200 μm.
- 6. the double threeway capillary pipe spray devices of open type according to claim 5, it is characterised in that：The capillary pipe spray The front end of pipe (3) is arranged in second three-way pipe (2), between the right-hand member of the horizontal tube of second three-way pipe (2) Distance is 1~3cm；The right-hand member of the horizontal tube of second three-way pipe (2) between the injection port of the mass spectrograph (9) away from From for 2~4cm.
- 7. the double threeway capillary pipe spray devices of open type according to claim 6, it is characterised in that：In the isocon (4) flow control valve is provided with.
- Examined 8. the double threeway capillary pipe spray devices of open type described in any one in claim 1~7 are analyzed in spray product Application in survey.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710881280.5A CN107833821B (en) | 2017-09-26 | 2017-09-26 | Open-type double-tee capillary spraying device and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710881280.5A CN107833821B (en) | 2017-09-26 | 2017-09-26 | Open-type double-tee capillary spraying device and application thereof |
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| Publication Number | Publication Date |
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| CN107833821A true CN107833821A (en) | 2018-03-23 |
| CN107833821B CN107833821B (en) | 2021-09-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710881280.5A Active CN107833821B (en) | 2017-09-26 | 2017-09-26 | Open-type double-tee capillary spraying device and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109559971A (en) * | 2018-11-14 | 2019-04-02 | 北京师范大学 | A kind of ionization apparatus and its application |
| CN109860015A (en) * | 2019-02-28 | 2019-06-07 | 苏州大学 | A kind of composite ionization source device |
| CN109950126A (en) * | 2019-03-18 | 2019-06-28 | 上海慧多信息科技发展有限公司 | A kind of unicellular electrospray ionization mass spectrum device of high throughput and its detection method |
| CN110455972A (en) * | 2019-08-21 | 2019-11-15 | 哈尔滨阿斯顿仪器有限公司 | Analysis method associated with a kind of liquid chromatography mass and its use interface arrangement |
| CN112368799A (en) * | 2018-05-03 | 2021-02-12 | 珀金埃尔默健康科学加拿大股份有限公司 | Ion generator for multiple gas flow |
| CN113176325A (en) * | 2021-04-14 | 2021-07-27 | 北京师范大学 | Normal-pressure mass spectrum online monitoring system for accelerated degradation of organic pollutants by plasmas in millisecond |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112368799A (en) * | 2018-05-03 | 2021-02-12 | 珀金埃尔默健康科学加拿大股份有限公司 | Ion generator for multiple gas flow |
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| CN109950126A (en) * | 2019-03-18 | 2019-06-28 | 上海慧多信息科技发展有限公司 | A kind of unicellular electrospray ionization mass spectrum device of high throughput and its detection method |
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| CN113176325A (en) * | 2021-04-14 | 2021-07-27 | 北京师范大学 | Normal-pressure mass spectrum online monitoring system for accelerated degradation of organic pollutants by plasmas in millisecond |
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